The
cyclotriphosphazene-substituted diazoacetate homopolymer (polyPNDA′)
(PNDA′ = hexaphenoxy-substituted phosphazene-containing methylene)
and a novel poly(substituted methylene) block copolymer, polyPNDA′-block-poly(hexyloxycarbonylmethylene) (polyPNDA’-b-polyHDA′), were synthesized, and the self-assembly
behavior of these polymers was studied in detail. A hexagonally packed
aggregated structure was observed in the self-assembled structure
of polyPNDA′, whereas a lamellar structure was observed in
the microphase-separated nanoassembly of polyPNDA′-b-polyHDA′. These results indicate that a hierarchical
structure composed of highly regular polyPNDA′ nanoaggregates
and the long-range microphase-separated polyPNDA′ and polyHDA′
domains had formed.